The application of headspace solid phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) was developed for the analysis of fenitrothion residues in wheat samples. Solid phase microextraction (SPME) is a new sample preparation technique that is fast, selective, low cost and environmental friendly. The SPME procedure was performed using a polydimethylsiloxane (PDMS) extraction fiber. Recovery studies were carried out at the two fortification levels; 0.1 mgkg-1 and 1 mgkg-1, and the average recoveries on the stablished levels were 98.9% and 101.2%. A good linearity (R2=0.95) was observed in the examined concentration range with standard deviation (SD) values. The limit of detection (LOD) was estimated as 0.01 mgkg-1. Also, a comparison of measured concentrations with codex maximum residue limits (MRLs) was performed. This method was applied successfully for fenitrothion residue determination in wheat samples.
